Synthesis and characterizations of alkaline, alkaline earth and transition metal borophosphate compounds
Alkali, toprak alkali ve geçiş metalleri borfosfat bileşiklerinin sentez ve karakterizasyonları
- Tez No: 93248
- Danışmanlar: PROF. DR. MERAL KIZILYALLI, PROF. DR. RUDİGER KNİEP
- Tez Türü: Doktora
- Konular: Kimya, Chemistry
- Anahtar Kelimeler: Borophosphates, hydrothermal synthesis, Rietveld analysis, zeotype, open- framework, porous compounds and magnetism
- Yıl: 2000
- Dil: İngilizce
- Üniversite: Orta Doğu Teknik Üniversitesi
- Enstitü: Fen Bilimleri Enstitüsü
- Ana Bilim Dalı: Kimya Ana Bilim Dalı
- Bilim Dalı: Belirtilmemiş.
- Sayfa Sayısı: 191
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Özet (Çeviri)
ABSTRACT SYNTHESIS AND CHARACTERIZATIONS OF ALKALINE, ALKALINE EARTH AND TRANSITION METAL BOROPHOSPHATE COMPOUNDS Yılmaz, Ayşen Ph.D., Department of Chemistry Supervisor: Prof. Dr. Meral Kızılyallı Co-supervisor: Prof. Dr. Rudiger Kniep September 2000, 168 pages In this thesis several synthesis methods and different compounds of alkaline, alkaline earth and transition elements were employed to explore and characterize new borophosphate compounds. For this purpose hydrothermal, high temperature solid state and boron flux methods were used. The hydrothermal reaction using Na2O.B2O3.P2O5 system produced NasB2P30i3, pentasodium catena-(diborato-triphosphate) in the powder form. The Rietveld analysis using GSAS software was applied for structural analysis and the data obtained were in good agreement with the single crystal data, 111which was published before. Atomic coordinates and selected bond lengths and angles are calculated and the x-ray powder data together with hkl Miller indices were given for first time in this work. The IR spectrum verifies the presence of BO4 and PO4 tetrahedra, which share common vertices. The hydrothermal reaction boron compounds with BaCb produced Ba2B2P20io in the powder form. The hydrothermal reactions with CaCb, gave hydroxy apatite, Ca5(P04)3(OH). On the other hand sodium version of CaBP05 and SrBP05, Na2BP05, was obtained by solid state reactions. A novel compound C03PPO7] was prepared by 5 different solid state reactions. Single crystals of C03P3PO7] were obtained by boron flux method and characterized by single-crystal diffraction data. The compound crystallizes in the monoclinic space group Cm with a=9.774(2), b=12.688(2), c=4.9057(8) Â, p=l 19.749(2)°; V=528.20(15) (Â3); Z=4. The structure consists of Co in trigonal bipyramids, square pyramids and distorted octahedra with isolated triangular B centers and tetrahedral P units. The temperature dependence of the magnetic susceptibility of the compound follows the Curie- Weiss law up to 3 OK. Below this temperature, the magnetic behaviour displayed first antiferromagnetic ordering followed by ferromagnetic coupling at 25K. Using the hydrothermal reactions of (NîL^HPC^, H3BO3 and H3PO4 with FeCİ2, a very interesting new borophosphate compound Fe(H20)2BP20g.H20 was obtained which was a rare ordered zeotype hydrated ferriborophosphate. The ordered, IV UMMSfiMAHTASYOK RfflRKEEEalternating, vertex-sharing B04ı PO4 and Fe04(H20)2 groups in Fe(H20)2BP20g.H20 form helical channels along the c axis. The framework is neutral and the magnetic susceptibility data is consistent with the oxidation state of Fe in the framework. Single Crystal data: Mw=3 10.65, hexagonal, space group P6522 (No: 179), a=9.4583(8) Â, c=15.707(2) Â, V=1216.9 Â3, Z=6, R=3.01%, Rw=7.50%. On the other hand in numerous experiments some new and pure compounds of other transition metals (Mn, Ni, Cu) and alkaline earth metals were found.
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